CN109406425A - For detecting detection agent of chlorine dioxide and preparation method thereof and detection method in water - Google Patents

For detecting detection agent of chlorine dioxide and preparation method thereof and detection method in water Download PDF

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Publication number
CN109406425A
CN109406425A CN201811343411.5A CN201811343411A CN109406425A CN 109406425 A CN109406425 A CN 109406425A CN 201811343411 A CN201811343411 A CN 201811343411A CN 109406425 A CN109406425 A CN 109406425A
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chlorine dioxide
indicator
water
preparation
sodium
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马丽
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Shanghai Leici Environmental Engineering Co., Ltd.
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INESA SCIENTIFIC INSTRUMENT CO Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

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  • Chemical & Material Sciences (AREA)
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  • Spectroscopy & Molecular Physics (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The present invention provides detection agent of chlorine dioxide content in a kind of detection water and preparation method thereof and detection methods.It is a kind of for detecting the detection agent of chlorine dioxide in water, which is characterized in that including reagent A and reagent B, the reagent A is indicator, and the indicator is the mixed liquor containing 1.1g/L anhydrous DPD sulfate and 2g/L EDETATE SODIUM;The reagent B is chlorine dioxide buffer, and the chlorine dioxide buffer is the mixed liquor of sodium citrate containing 1mol/L, 1mol/L sodium hydroxide and 2% glycine.

Description

For detecting detection agent of chlorine dioxide and preparation method thereof and detection method in water
Technical field
The present invention relates to a kind of detection techniques of chlorine dioxide content in water, can be used for chlorine dioxide in colorimetric method measurement water Content, belong to chemical analysis technology field.More particularly to it is a kind of for detect in water the detection agent of chlorine dioxide content and its Preparation method and detection method.
Background technique
Currently, all centralized water supplies of national requirements, output water all should be sterile-processed, output water and Terminal tap water The surplus of middle disinfectant should all meet standard GB/T 5749-2006 " standards for drinking water quality ".Disinfection to water sterilization There are many agent type, and traditional disinfectant has chlorine or liquid chlorine etc., and emerging then have chlorine dioxide, ozone, ultraviolet light etc..Accordingly Ground, chlorine residue in water, total chlorine, chlorine dioxide content be the important indicator of monitoring control water disinfection effect.
In the prior art, the detection method of chlorine residue, total chlorine and chlorine dioxide has: chemical method (including iodimetric titration, N, N- diethyl Base-Isosorbide-5-Nitrae-phenylenediamine (DPD) ferrous ammonium sulfate titration etc.), spectrophotometry, electrochemistry and residual chlorine sensor method etc., wherein More common is N, N- diethyl -1,4- phenylenediamine (DPD) spectrophotometry.
The principle of N, N- diethyl -1,4- phenylenediamine (DPD) spectrophotometry measurement chlorine dioxide are as follows: glycine will be in water Free chlorine be converted into hydrargyrum amidochloratum acetic acid without interfere chlorine dioxide measurement, pH be 6.2~6.5 under conditions of, dioxy Change chlorine and N, N- diethyl-Isosorbide-5-Nitrae-phenylenediamine (DPD) to react, generate red compound, under 515nm wavelength, using point Light photometry measures its absorbance, measures chlorine dioxide.
According to national standard GB/T5750.11-2006 " Drinking Water water examination Disinfection Methods agent index ", chlorine dioxide Test agent need to be configured to certain density liquid, then be measured, wherein DPD color developing agent must be stored in after being made into liquid It in brown bottle, and in being saved in refrigerator, otherwise will soon fail, influence the accuracy of measurement.
Summary of the invention
Technical problem to be solved by the present invention lies in the above-mentioned deficiencies overcome in the presence of existing test method, provide one Kind to preservation condition require it is lower, with good using effect for N, N- diethyl -1,4- phenylenediamine (DPD) spectrophotometric Method detects the detection agent of chlorine dioxide in water.
Its technical problem to be solved can be implemented by the following technical programs.
It is a kind of for detecting the detection agent of chlorine dioxide in water, including reagent A and reagent B,
The reagent A is indicator, and the indicator is containing the anhydrous DPD sulfate of 1.1g/L and 2g/L EDETATE SODIUM Mixed liquor;
The reagent B is chlorine dioxide buffer, and the chlorine dioxide buffer is sodium citrate containing 1mol/L, 1mol/L The mixed liquor (containing glycine 2g in i.e. every 100ml final solution) of sodium hydroxide and 2% glycine.
Another technical problem to be solved by this invention is to provide a kind of for detecting the detection agent of chlorine dioxide in water Preparation method, which includes the following steps:
A), the preparation of indicator
A1), the preparation of indicator solvent
The sulfuric acid solution for preparing 1mol/L is spare as indicator solvent;
A2), the preparation of indicator pulvis
By every liter of solution containing the concentration of the anhydrous DPD sulfate of 1.1g and 2g EDETATE SODIUM weigh anhydrous DPD sulfate and EDETATE SODIUM, it is spare as indicator pulvis after mixing;
A3), the preparation of indicator
The indicator pulvis for taking step a2 to obtain is dissolved in appropriate step a1 in obtained indicator solvent, is configured to Mixed liquor containing 1.1g/L anhydrous DPD sulfate and 2g/L EDETATE SODIUM;It is kept in dark place;
B), the preparation of chlorine dioxide buffer
Sodium citrate and sodium hydroxide are weighed in the ratio of every liter of solution 294.1g containing sodium citrate, sodium hydroxide 40g, is used Newly boil without room temperature is cooled to after chlorine water dissolution, and be settled to setting capacity, be prepared into sodium citrate containing 1mol/L and 1mol/L The mixed liquor of sodium hydroxide is spare as chlorine residue buffer;
Glycine is dissolved in the chlorine residue and caches liquid by the ratio that 20g glycine is corresponded in chlorine residue buffer described in every 1L In, it mixes, obtains chlorine dioxide buffer.
Wherein, it in step a1, is slowly added in 800mL water using by the concentrated sulfuric acid 55.0mL of ρ=1.84g/mL, is cooled to room Wen Hou, then be settled to the adding proportion of 1000mL and complete the preparation of the indicator solvent.
As the preferred embodiment of the present invention, in the step c, the preparation of the chlorine dioxide caching liquid is most better than described Chlorine dioxide buffer is completed before use.
Another technical problem to be solved by this invention is to provide chlorine dioxide in a kind of aforementioned detection agent detection water Method, the detection method include the following steps:
Water sample to be measured and the indicator and the chlorine dioxide buffer are mixed by the volume ratio of 10:1:1,2min It is interior to use spectrophotometer or colorimetric measurements.
Wherein, measurement absorbance at spectrophotometer 515nm is included in using the spectrophotometer measurement, calculates dioxy The step of changing cl concn.
With N, N- diethyl-Isosorbide-5-Nitrae-phenylenediamine (DPD) spectrophotometry, detection agent and its inspection by adopting the above technical scheme When survey method measures chlorine dioxide in water, the problem of DPD color developing agent is unable to long-term preservation at room temperature can effectively solve the problem that.
Specific embodiment
The present invention includes indicator, chlorine dioxide buffer.
Indicator includes indicator solvent and indicator pulvis again, dissolves the two mix before use, and be stored in brown bottle In.Indicator solvent is about 1mol/L sulfuric acid solution;Indicator pulvis is anhydrous DPD sulfate and EDETATE SODIUM, with indicator Solvent is configured to the mixed liquor containing 1.1g/L anhydrous DPD sulfate and 2g/L EDETATE SODIUM.
Chlorine dioxide buffer is the mixed liquor of sodium citrate containing 1mol/L, 1mol/L sodium hydroxide and 2% glycine, is faced Three is mixed with preceding.
When measurement, water sample to be measured and indicator and chlorine dioxide buffer are mixed in the ratio of 10:1:1, used in 2min Spectrophotometer or colorimetric measurements.
A specific embodiment of the invention is described in further detail below in conjunction with embodiment.
A), the preparation of indicator
I. the preparation of indicator solvent
The 55.0mL concentrated sulfuric acid (ρ=1.84g/mL) is slowly added in 800mL water, after being cooled to room temperature, is settled to 1000mL.
Ii. the preparation of indicator pulvis
The anhydrous DPD sulfate of 1.1g and 2g EDETATE SODIUM are weighed, is mixed.
Iii. the preparation of indicator
Before use, indicator pulvis is dissolved in indicator solvent, is stored in brown bottle.
B), the preparation of chlorine dioxide buffer
294.1g sodium citrate and 40g sodium hydroxide are weighed, is cooled to room temperature, and constant volume after being dissolved with what is newly boiled without chlorine water It is spare to 1000mL.
20g glycine is weighed, is dissolved in the above-mentioned solution of 1000mL before use, is mixed.
C), the measurement of chlorine dioxide:
Take the tap water of 5mL disinfection by chlorine dioxide in colorimetric cylinder, be separately added into 0.5mL chlorine dioxide buffer and 0.5mL indicator, covers tightly colorimetric cylinder lid, and shaking colorimetric cylinder makes its mixing, in 2min, the measurement suction spectrophotometer 515nm at Luminosity calculates chlorine dioxide concentration.

Claims (6)

1. a kind of for detecting the detection agent of chlorine dioxide in water, which is characterized in that including reagent A and reagent B;
The reagent A is indicator, and the indicator is the mixing containing 1.1g/L anhydrous DPD sulfate and 2g/L EDETATE SODIUM Liquid;
The reagent B is chlorine dioxide buffer, and the chlorine dioxide buffer is sodium citrate containing 1mol/L, 1mol/L hydrogen-oxygen Change the mixed liquor of sodium and 2% glycine.
2. a kind of for detecting the preparation method of the detection agent of chlorine dioxide in water, which comprises the steps of:
A), the preparation of indicator
A1), the preparation of indicator solvent
The sulfuric acid solution for preparing 1mol/L is spare as indicator solvent;
A2), the preparation of indicator pulvis
Anhydrous DPD sulfate and EDTA bis- are weighed containing the concentration of the anhydrous DPD sulfate of 1.1g and 2g EDETATE SODIUM by every liter of solution Sodium, it is spare as indicator pulvis after mixing;
A3), the preparation of indicator
The indicator pulvis for taking step a2 to obtain is dissolved in appropriate step a1 in obtained indicator solvent, is configured to contain The mixed liquor of 1.1g/L anhydrous DPD sulfate and 2g/L EDETATE SODIUM;It is kept in dark place;
B), the preparation of chlorine dioxide buffer
Sodium citrate and sodium hydroxide are weighed by the concentration of every liter of solution 294.1g containing sodium citrate, sodium hydroxide 40g, with newly boiling Boiling without room temperature is cooled to after chlorine water dissolution, and be settled to setting capacity, be prepared into sodium citrate containing 1mol/L and 1mol/L hydrogen-oxygen The mixed liquor for changing sodium is spare as chlorine residue buffer;
Glycine is dissolved in the chlorine residue caching liquid, mixes by the ratio that 20g glycine is corresponded in chlorine residue buffer described in every 1L It is even, obtain chlorine dioxide buffer.
3. using the preparation method for being used to detect the detection agent of chlorine dioxide in water described in claim 2, which is characterized in that step It in a1, is slowly added in 800mL water using by the 55.0mL of ρ=1.84g/mL concentrated sulfuric acid, after being cooled to room temperature, then is settled to The adding proportion of 1000mL completes the preparation of the indicator solvent.
4. using the preparation method for being used to detect the detection agent of chlorine dioxide in water described in claim 2, which is characterized in that described In step b, the chlorine dioxide buffer that is formulated in of the chlorine dioxide buffer is completed before use.
5. a kind of method using chlorine dioxide in the detection water of detection agent described in claim 1, which is characterized in that including walking as follows It is rapid:
Water sample to be measured and the indicator and the chlorine dioxide buffer are mixed by the volume ratio of 10:1:1, used in 2min Spectrophotometer or colorimetric measurements.
6. the method that detection agent detects chlorine dioxide in water according to claim 5, which is characterized in that use the light splitting light The step of degree meter measurement is included in measurement absorbance at spectrophotometer 515nm, calculates chlorine dioxide concentration.
CN201811343411.5A 2018-11-13 2018-11-13 For detecting detection agent of chlorine dioxide and preparation method thereof and detection method in water Pending CN109406425A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110161026A (en) * 2019-06-14 2019-08-23 安徽理工大学 The centrifugal type microfludic chip of chlorine residue in a kind of DPD spectrophotometry water
CN111504992A (en) * 2020-05-06 2020-08-07 中国检验检疫科学研究院 Rapid detection kit for chlorine dioxide after ballast water disinfection
EP3767289A1 (en) * 2019-07-18 2021-01-20 AXAGARIUS GmbH & Co. KG Test device and method for semi-quantitative determination of chlorine dioxide in a liquid sample containing free chlorine

Citations (5)

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Publication number Priority date Publication date Assignee Title
CN101241080A (en) * 2008-01-25 2008-08-13 黄晓平 Convenient colorimetric technique for detecting subaqueous polymorphic chlorine and its color comparator
CN102128833A (en) * 2010-12-31 2011-07-20 杨海宁 Reagent kit for detecting residual chlorine in water
CN104677900A (en) * 2015-02-28 2015-06-03 温州医科大学 Method capable of eliminating influence of reagent blank and rapidly detecting content of chlorine dioxide in water
CN105372194A (en) * 2015-12-16 2016-03-02 浙江大学昆山创新中心 Indicator of residual chlorine online detector, preparation and use method
CN105606554A (en) * 2016-03-07 2016-05-25 上海仪电科学仪器股份有限公司 Method for measuring free chlorine and total chlorine in water

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101241080A (en) * 2008-01-25 2008-08-13 黄晓平 Convenient colorimetric technique for detecting subaqueous polymorphic chlorine and its color comparator
CN102128833A (en) * 2010-12-31 2011-07-20 杨海宁 Reagent kit for detecting residual chlorine in water
CN104677900A (en) * 2015-02-28 2015-06-03 温州医科大学 Method capable of eliminating influence of reagent blank and rapidly detecting content of chlorine dioxide in water
CN105372194A (en) * 2015-12-16 2016-03-02 浙江大学昆山创新中心 Indicator of residual chlorine online detector, preparation and use method
CN105606554A (en) * 2016-03-07 2016-05-25 上海仪电科学仪器股份有限公司 Method for measuring free chlorine and total chlorine in water

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110161026A (en) * 2019-06-14 2019-08-23 安徽理工大学 The centrifugal type microfludic chip of chlorine residue in a kind of DPD spectrophotometry water
EP3767289A1 (en) * 2019-07-18 2021-01-20 AXAGARIUS GmbH & Co. KG Test device and method for semi-quantitative determination of chlorine dioxide in a liquid sample containing free chlorine
CN111504992A (en) * 2020-05-06 2020-08-07 中国检验检疫科学研究院 Rapid detection kit for chlorine dioxide after ballast water disinfection

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Address after: 201805 Room 101, Building 2, 111 Miquan Road, Anting Town, Jiading District, Shanghai

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